HRID2260048

反应详情

EQUATION

反应方程式

HRID 2260048 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 8.06 g portion of 3-amino-4-methyl-1H-pyrazole was dissolved in 30 ml of acetonitrile and, with cooling on an ice bath, 12.9 g of ethyl propionimidate hydrochloride was added to the solution. The resulting mixture was stirred for 1 hour at the same temperature and then overnight at room temperature. After removing insoluble materials by filtration, the resulting filtrate was concentrated under a reduced pressure, and the thus obtained residue was subjected to silica gel column chromatography. Elution with methanol-chloroform (1:9-3:7, v/v) gave 8.40 g of N-(4-methyl-1H-pyrazol-3-yl)propionamidine hydrochloride.

WORKUP

后处理

  1. temperaturewith cooling on an ice bath
  2. customovernight
  3. customat room temperature
  4. customAfter removing insoluble materials
  5. filtrationby filtration
  6. concentrationthe resulting filtrate was concentrated under a reduced pressure
  7. washElution with methanol-chloroform (1:9-3:7